工作场所空气中8种N-亚硝胺化合物测定的GC-MS/MS法
Determination of 8 N-nitrosamines in the workplace air by GC-MS/MS method
孟祥娟 1刘晓东 1张晓梅 1胡越 1郭启芬1
作者信息
- 1. 北京市化工职业病防治院中心实验室,北京 100093
- 折叠
摘要
目的 建立工作场所空气中N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基甲基乙胺、N-亚硝基二丁胺、N-亚硝基正丙胺、N-亚硝基吗啉、N-亚硝基二苯胺和N-亚硝基吡咯烷8种N-亚硝胺化合物的气相色谱-串联质谱(GC-MS/MS)检测方法.方法 于2023年1至8月,以ThermoSorb/N柱采集工作场所中空气中8种N-亚硝胺,用4 ml甲醇-二氯甲烷(体积比1:1)溶液解吸,VF-624ms毛细管色谱柱分离,多反应监测模式检测,外标法定量,并对方法的检出限和精密度等指标进行分析.结果 8种N-亚硝胺测定方法的线性范围为1.0～20.0 µg/L,相关系数0.999 3～0.999 9,方法检出限0.051～0.132μg/L,最低定量浓度0.030～0.078 µg/m3(以空气体积22.5 L,解吸液体积4.0 ml计),批内精密度2.05％～6.89％,批间精密度2.41％～8.26％,解吸效率67.20％～102.60％;样品在4℃条件下至少可保存7 d.结论 GC-MS/MS测定工作场所空气中8种N-亚硝胺方法的灵敏度高、精密度好,可准确测定工作场所空气中8种N-亚硝胺含量.
Abstract
Objective To establish a method for the determination of eight N-nitrosamines(N-nitrosodimethylamine,N-nitrosodimethylamine,N-nitrosomethylmethylamine,N-nitrosodibutylamine,N-nitrosopropylamine,N-nitrosomorpholine,N-nitrosodianiline and N-nitrosopiperidine)in the air of workplace by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods From January to August 2023,eight N-nitrosamines in the air of workplace were collected by ThermoSorb/N column,eluted with 4 ml methanol-dichloromethane(1:1 volume ratio),separated by VF-624 ms capillary column,detected by multiple reaction monitoring mode and quantified by external standard method.The detection limit and precision of the method were also analyzed.Results The linear range of the method for the determination of eight N-nitrosamines was 1.0-20.0 μg/L,the correlation coefficient was 0.9993-0.9999,the detection limit was 0.051-0.132 μg/L,and the minimum quantitative concentration was 0.030-0.078 µg/m3(calculated by collecting 22.5 L of air sample and eluting with 4.0 ml stripping liquid).The within-run precisions were 2.05％-6.89％and the between-run precisions were 2.41％-8.26％.The desorption rates were 67.20％-102.60％.The sample can be kept at least 7 days at 4 ℃.Conclusion GC-MS/MS method for the determination of eight N-nitrosamines in workplace air has high sensitivity and good precision,and can accurately determine the content of eight N-nitrosamines in workplace air.
关键词
气相色谱-质谱法/串联质谱法/N-亚硝胺/工作场所/空气Key words
Gas chromatography-mass spectrometry/Tandem mass spectrometry/N-nitrosamines/Workplace/Air引用本文复制引用
出版年
2024
NETL
NSTL
万方数据